Leavening composition



Patented Jan. 9,

Rudolph I. Hui-ta, Clearwater, Fla, asslgnor to Monsanto Chemical Company, a corporation of Delaware No Drawing. Application July, 1942,

Serial No. 451,499

20 Claims. (01. 99-95) v This invention relates to improved chemical leavening agents of the calcium pyrophosphate ype.

The invention herein disclosed and claimed is an improvement particularly upon the invention disclosed and claimed in the application of Charles F. Booth, Serial No. 335,840, filed May 17,

1940. It may however be applied to other calcium acid pyrophosphate containing compositions.

The process disclosed-in the Booth application consists in the reaction together of phosphoric acid and a lime base such as quick lime under conditions so that a temperature substantially above 140' C. and preferably above 180 C., but below 300 C., is attained in the reacting mass. The product obtained by the'Booth process comprises crystallized calcium acid pyrophosphate, CaHzPzQntogether with monocalcium orthophos- V phate, the calcium acid pyrophosphate comprising upwards of 20% of the mixture. According to the Booth process calcium acid pyrophosphate leavening compositions may be prepared by variations in the procedure therein described and products produced thereby which contain upwardly of 20% crystallized calcium acid pyrophosphate and specifically. from 50% through 60% upwards to 90% of this compound.

I Since the Booth product is produced by a process wherein simultaneous crystallization of both calcium acid pyrophosphate and monocalcium orthophosphate takes place, the product is presumably an inter-crystalline association of these two compounds and it is believed that the relatively high leavening activity of this mixture of compounds is due to the fact that either the calcium acid pyrophosphate is activated by the mdnocalcium orthophosphate or that the product by virtue of its process of manufacture contains "activating" water ina minor amount, that is, :vater not chemically bound as water of hydraion.

The compound, calcium'acid pyrophosphate, CaHzPzOv, may also be prepared by heating either the hydrated or anhydrous monocalcium 'orthophosphate, CB.H4(PO4) 2, to temperatures at which moleculariy combined water is liberated. By variations in the degree and method of heating products may be obtained which contain varying amounts of the acid pyrophosphate and orthophcsphate, or which comprise particles or crystals oi monocalcium orthophosphate carrying acoatin: of calcium acid pyrcphosphate. Various rates or reaction may be obtained by mechanically mixing either thermally produced or crystallized calcium acid pyrophosphate together with monocalscium orthophosphat of either the hydrated or anhydrous variety. The anhydrous variety of monocalcium orthophosphate may for this pur-' pose be produced in either the solid crystalline or in the porous condition.

A method of evaluating chemical leavening agents of the herein' described type is described in the Journal of Cereal Chemistry, vol. 8 at page 423, 1931. This method has been adopted as a Standard biscuit baking test by the American Association of Cereal Chemists. In the procedure as adopted by this association, in order. to eliminate uncontrollable variables, it is customary to employ water as the liquid when preparing the biscuit dough. When preparing biscuit doughs using the leavening agent prepared by any of the aforesaid methods and employing water as the liquid, as called for by the Standard baking procedure, satisfactory biscuits are obtained. However, when employing milk as the liquid for making the dough, certain adverse effects are encountered which, it is believed, are caused by the effect of calcium acid pyrophosphateor ions formed therefrom upon the milk or constituents thereof such as proteins. Such adverse eiiect is recognized by the so-called "short deughs, the

elasticity of which has been seriously reduced.

In investigating the effect of this adverse result when employing milk as the liquid in biscuit manufacture, I have discovered that the adverse eflect is more pronounced when chemically bleached flours are employed than when unbleached fiours are used. a

The adverse effect of the calcium acid pyrophosphate leavening in the presence of milk, upon biscuits may be measured by the standard biscuit baking technique and is illustrated in Table I below, which gives data taken from actual biscults which have been baked utilizing a calcium acid pyrophosphate leavening with the three fluids; water, reconstituted dried skim milk, and

ireshmilk.

Table I Wt. Actual Specific PH dough volume volume 1 dram-Eloy. 1.0a 25.8 .a 18.93 2 C. A. P. P.+dried skim milk 6.87 23.8 55.0 17.40 3 G.A.P.P+freshmilk- 6.94 24.3. 57.8 17.72

As will be noted from the table, the eiiect of, the calcium acid pyrophosphate, designated as C. A. P. P. in the table, when employing milk is manifested by a slightly lower pfland a. lower specific volume of the biscuit. This effect is encountered both with the dried skim milk and with 1 have now found that by the addition to the calcium acid pyrophosphate leavening agent of a glassy soluble alkali metal metaphosphate, more particularly the glassy sodium hexa metaphosphate, commonly known as Graham's salt, the adverse effect pointed out above can be substantially overcome. For the purpose of realizing the improved results it is necessary only that the sodium hexa metaphosphate be present during the leayening reaction, that is, at the time when the liquid is added to the dry constituents, to form the dough. For this purpose I may accordingly prepare a mixture of the calcium acid pyrophosphate and the sodium hexa metapho sphate by preparing both salts in the finely divided or powdery state and then thoroughly mixing the two salts together. It is also practical to dissolve the sodium hexa metaphosphat or other soluble metaphosphate in the liquid, that is, in the water or in the milk which is employed for the biscuit dough. For the preparation of baking powders where all constituents are thoroughly mixed together in the form of a more or less fine powder, I prefer to powder the Grahams salt to at least the same fineness as the other constituents of the baking powder and mix it thoroughly therein. For the preparation of self-rising flours I prefer to first produce a mixture of phosphates, that is, the calcium acid pyrophosphate, as it is disclosed in the Booth application, and mix therewith the sodium hexa metaphosphate or Graham's salt generally in the proportions of 6 parts by weight of the calcium acid pyrophosphate to 1 part of the soluble sodium hexa metaphosphate. These proportions may be somewhat varied, and in general I have found that usually from 1 part of the soluble metaphosphate to as much as 10 to 12 parts, or to aslittle as 3 to 4 parts of calcium acid pyrophosphate may be used. For the preparation of self-rising flours the crystallized calcium acid pyrophosphate-sodium metaphosphate mixture is incorporated into the fiour in the usual proportions, that is, per 1,000 parts of flour I employ 15 to parts of phosphate, together with sumcient sodium bicarbonate to produce with the phosphate mixture a substantially neutral biscuit.

In place of sodium hexa metaphosphate I may employ a mixture of sodium and potassium metaphosphate. Such a mixture is preferably made tions of the corresponding orthophosphate salts. Baked products using my improved leavening composition have a somewhat improved taste, that is, the calcium acid pyrophosphate taste has'been substantially eliminated, the color of the baked product is somewhat better and the biscuit is considerably lighter.

Illustrating the eiiect of my composition uponaaeasm baked products, the results in Table II, we. ob-

tained utilizing the standard biscuit baking pro cedure, and employing a 4 minute delay between mixing and rolling the dough, in order to accentu- A"=sodiuin hexa metaphosphate, Graham's salt. "B" -mixture consisting oi 80% NaP0i+20% KPO: which has been fused and quickly cooled.

From the above table it will be noted that biscuits baked with doughs leavened with calcium acid pyrophosphate and containing sodium hexa metaphosphate or a potassium metaphosphate containing mixture in amount equivalent to 0.5%

based upon the dry ingredients of the dough, are

pared by fusion utilizing the equivalent proporsubstantially lighter than when such sodium metaphosphate is absent from the dough. It will also be noted that either milk or water may be used as the liquid forforming the dough without sacrifice of lightness of the biscuit or elasticity of the dough.

Tests made in a commercial bakery on so-called high sugar ratio white cakes showed that C. A. P. P. containing a minor proportion of the alkali metal metaphosphate producedcakes which possessed preferred characteristics shown in the following table:

. Table Ill 0.x. P P (1A.? P.

Symmetry Y 14.3 16.0 Actual volume. 672 692 Specific volume .cc.lg.. 3. 23 5. 2t

C=mixture consisting of 90.5% fiaP0i+9.5% KPOa.

The mixtures of calcium acid pyrophosphate and sodium metaphosphate-herein disclosed are loose mixtures in the ordinary sense of theterm.

There is, in other words, no coating of the crystals /or particles of the calcium pyrophosphate by means of the sodium metaphosphate or other metaphosphate employed. Where coatings have been employed in the past, particularly upon anhydrous monocalcium phosphate, such coatings have been described as alkali metal metaphosphates. However, due to the method of preparation ofthe prior art products these coatings are not theequivalent of the hexa metaphosphates or Graham's salt herein employed, primarily because the coating salts were insoluble, and consequently had no eifect upon the proteins of milk in the presence ofpyrophos'phate. What I claim is: I

1. A leavening acid comprisingcalcium acid pyrophosphate and a minor proportion of analkali metal hexa metaphospnate. 2. A leavening acid comprising calcium acid pyrophosphate and a minor. proportion of sodium hexa metaphosphate.

3. A leavening acid comprising an intercrystal line mixture of calcium acid pyrophosphate,-

monocalcium. orthophosphate and-a minor proportion of glassy sodium metaphosphate.

4. A leavening acid comprising a mixture oi calcium acid pyrophosphate and monocalcium orthophosphate, said mixture consisting of from 20% to 90% of calcium acid pyrophosphate and said acid containing a minor proportion of soluble glassy sodium metaphosphate.

5. The acid defined in claim 4 in which the acid contains from 5 to 12 parts of calcium acid pyrophosphate for each part of sodium meta phosphate.

6. The acid defined in claim 4 in whichthe dium bicarbonate. calcium acid Dyrophosphate' sodium metaphosphate contains suflicient potas sium salt to render the sodium metaphosphate substantially non-hygroscopic.

7. The leavening' acid defined in claim 4 in which the sodium metaphosphate contains from 10% to 20% of potassium salt.

8. A leavening acid comprising monocalcium phosphate particles carrying a coating of calcium acid pyrophosphate,.said acid including a minor proportion of glassy soluble sodium metaphosphate.

9. The acid defined by claim 4 in which the.

glass soluble sodium metaphosphate contains a minoramount of potassium metaphosphate' 10. A leavening acid comprising calcium acid pyrophosphate, and a minor proportion of a soluble glassy metaphosphate, the basic constituent of said metaphosphate being an alkali oxide.

11. A leavening acid comprising a mixture of calcium acid pyrophosphate and monocalcium orthophosphatasaid mixture consisting oi from 20% to 90% of calcium acid pyrophosphate, said mixture also containing a soluble glassy metaphosphate, the basic constituent of said metaphosphate being an alkali oxide.

12. In a method of leavening in which sodium bicarbonate is reacted with calcium acid pyrophosphate in a liquid medium containing milk.

the improvement which comprises carrying out said reaction in the presence of soluble glassy sodium metaphosphate.

13. The method defined in claim 12 in which the leavening reaction is carried out in the presence oi dissolved sodium hexa metaphosphate.

14 A leavening composition comprising soand a minor proportion of sodium hexa metaphosphate.

15. A leavening composition comprising sodium bicarbonate calcium acid pyrophosphate and a minor proportion of a glassy soluble alkali metal metaphosphate.

16. A leavening composition comprising sodium bicarbonate. calcium acid pyrophosphate and a minor proportion of an alkali metaphosphate.

17. A baking preparation comprising flour, so-

dium bicarbonate, calcium acid pyrophosphate and a minor proportion 01 a soluble alkali metal metaphosphate.

18. A baking preparation comprising flour, sodium bicarbonate, calcium acid pyrophosphate and a minorpropo'rtion of a soluble glassy a1- kaii metal metaphosphate.

19. Abaking preparation comprising flour, sodium bicarbonate, calcium acid pyron and a minor proportion of sodium hexa metaphosphate.

20. In a method of lea'vening in which sodium bicarbonate is reacted with calcium acid pyrophosphate ina liquid medium containing milk. the improvement which comprises carrying out said reaction in the presenceof an alkali metal hexa'metaphosphate. v

- RUDOLPH J. HURKA.

metal hexa 

